Bull. Mater. Sci.

(2018) 41:28 © Indian Academy of Sciences

[Link]

Development and properties of advanced composites based on cork

and nanometric silicon carbide-filled phenolic resin

G PELIN1,2,∗ , C-E PELIN1 , A ŞTEFAN1 , I DINCĂ1 , E ANDRONESCU2 , O OPREA2 , D FICAI2

and R TRUŞCĂ2
1 MaterialsUnit, National Institute for Aerospace Research ‘Elie Carafoli’, 061126 Bucharest, Romania
2 Facultyof Applied Chemistry and Materials Science, Politehnica University of Bucharest,
011061 Bucharest, Romania
∗ Author for correspondence ([Link]@[Link], [Link]@[Link])

MS received 8 July 2016; accepted 26 October 2017

Abstract. This paper presents the obtaining of advanced materials based on cork powder as reinforcement and phenolic
resin (PR) with silicon carbide (nSiC) nanofiller as matrix with potential applications in aerospace industry. Three for-
mulations were obtained: one control sample PR/cork with no nanofiller, two nanofilled samples with 1 and 2 wt% nSiC
loadings into the resin. The materials were tested by flexural and compressive mechanical tests to determine their strength
and stiffness, to determine their friction coefficient by tribological tests, to determine their thermal decomposition behaviour
by TG-DSC analysis and to evaluate their thermal behaviour by thermal shock tests when subjected to extreme temperature
directly from room temperature. The material structure was analysed by SEM visualizing the fracture cross-section after
mechanical testing. The test results illustrate that silicon carbide nanoparticles improve flexural and compressive strength,
but also stiffness and friction coefficient, delay thermal decomposition onset and improve thermal shock resistance. All these
sustain the PR/nSiC/cork materials as potential advanced materials candidates for thermal protection applications.

Keywords. Cork phenolic; silicon carbide nanoparticles; thermal shock resistance; mechanical strength.

1. Introduction are heated as they penetrate towards the surface, transferring

energy from solid to gas phase [6].
Thermal protection systems (TPS) are key elements for Cork is one of the materials used for numerous space
prevention of excessive heat reaching the metallic structure in applications due to its intrinsic properties, such as thermal
spacecraft missions. There are two basic concepts of thermal resistance during reentry phase of space vehicles. Norcoat-
protection systems: reusable materials, i.e., carbon–carbon Liege is an ablative material consisting of composites based
composites and non-reusable, i.e., ablative materials (abla- on phenolic resin (PR) matrix with homogenized cork par-
tors). The selection of one of the two categories is done ticles [7], developed by European Aeronautic Defence and
based on the spacecraft mission and financial restrictions Space and used in the rear cone and back-cover section of
[1]. the atmospheric reentry demonstrator (ARD), a sub-orbital
Reusable systems, such as reinforced carbon–carbon mate- reentry vehicle launched in 1998 by European Space Agency
rials are generally used as low-weight tiles in wing-leading (ESA), that will also intend to use it in ExoMars mission
edges of space capsules, where temperature can exceed after some adaptation to meet the requirements specific for
1260◦ C [2]. For temperatures lower than 1200◦ C, materials Mars entry missions [8–10]. Besides ESA’s missions, cork
that are able to withstand several extreme thermal cycles are was used as insulator between the metal/Kevlar case and
generally used, these include alumina- or silica-based mate- the propellant in solid rocket boosters [11], and it is stud-
rials, C/SiC and Cf/SiC composites [2]. ied for other applications, such as high-performance aircraft
Ablative materials are generally designed for non-reusable structural composites. In this case, cork-filled epoxy com-
planetary probes, as they insulate a large heat amount through posites [12] and cork-filled carbon fibre-reinforced polymer
phase change, by resin decomposition process that generates (CFRP) laminates [13] with improved mechanical and impact
the absorption of a large part of this heat, and prevents it resistances were obtained. Cork was added to jute/epoxy com-
from passing to the next layer material [3]. The char layer posites to enhance thermal stability [14], and to EPDM rubber
formed after the resin degradation, acts as an insulator, while ablative composites to enhance thermal endurance and abla-
the material continues to decompose and outgas [4,5]. The tion characteristics [15]. Recent studies present the use of
nature of the process is endothermic and the pyrolysis gases cork as a compound in nanocomposites, aerogel/cork/silicone
28 Page 2 of 9 Bull. Mater. Sci. (2018) 41:28

nanocomposites were obtained by Raeisi et al [16], and

their results showed that cork pores were filled with aerogel
nanostructures and generated density increase and thermal
conductivity decrease. However, there are very few stud-
ies presenting cork phenolic composites modified with the
aid of nanofillers. Inorganic nanofillers such as nanometric
silicon carbide (nSiC), nano-silica, nanoclays, ZrB2 or BN
are promising filler reinforcement agents used to improve
processability, toughness, char yield as well as tribological
and thermal properties of PR matrix [17,18]. Amongst all
nanofillers, silicon carbide presents exceptional properties for
high-temperature applications of composites, i.e., oxidative
and thermal shock resistance and excellent friction proper-
ties [19], as shown in studies presented in literature [20–22].
One previous study conducted by the authors [23] showed
significant positive effect that nanometric SiC had on mechan-
ical, thermo-mechanical and tribological properties of PR Figure 1. Temperature treatment programme for curing process of
the PR/nSiC/cork composites.
as stand-alone material. As a continuation of this research,
the current study focussed on using the nSiC-filled PR com-
posites as matrix of cork-based ablative-type materials. The composition and decrease bubble formation in the bulk
current study presents the obtaining of ablative composites composites. The mixture was placed in a mould (covered with
based on cork and PR-filled with silicon carbide nanopar- a release agent) and the curing process was carried out accord-
ticles in different weight contents, the aim of the paper is ing to a programme in which temperature was increased in
the evaluation of the silicon carbide nanoparticles loading stages, as described in figure 1. The mould was placed in a
effect. The mechanical, tribological and thermal properties hydraulic press at 70◦ C and the temperature was increased by
show enhanced performance when silicon carbide nanopar- 20◦ C with dwell time of 20 min at each temperature step. In
ticles are present in the ternary composite, sustaining these the 90◦ C step, the pressing of the composites started, using
nanofilled materials as potential candidates for ablators with the pressure value of 3 kg cm−2 . Cooling took place under
enhanced properties for advanced applications. pressure down to room temperature.

2.3 Testing and characterization

2. Experimental
The materials were tested by mechanical, tribological and
2.1 Materials thermal tests. Prior to the nanocomposite obtaining process,
the liquid PR and nanofilled PR were subjected to viscos-
The resin used as matrix was resole PR ISOPHEN 215 ity measurements using Ubbelohde capillary tube viscometer
SM 57% provided by ISOVOLTA S.A. Bucharest, with (Cannon CT-1000). Mechanical testing was performed at
1.135 g cm−3 density. The material used as preform to be room temperature using INSTRON 5982 mechanical testing
impregnated with resin was cork powder with grain size machine and consisted of 3-point bending and compression
between 0.5 and 1 mm. β-type nSiC powder (97.5% purity, tests. 3-point bending tests were performed according to SR
34−40 m2 g−1 specific surface area and 3.22 g cm−3 true den- EN ISO 178 [24], at 2 mm min−1 testing speed and using
sity) purchased from Nanostructured & Amorphous Materials nominal span length (16× specimen thickness) on rectangular
Inc., USA, was used as nanofiller agent. specimens (80×15×4 mm) using five specimens per sample.
Compressive properties were measured according to ASTM D
2.2 Obtaining procedure 1074 [25] at 1.3 mm min−1 testing speed on cylindrical spec-
imens with 12.7 mm diameter and 4 mm height using five
The PR/nSiC/cork composites were obtained by following a specimens per sample. After mechanical testing, the fracture
multiple step procedure. For the nanofilled samples, nSiC was cross-section was analysed by scanning electron microscopy
added to the liquid PR in 2 weight contents relative to the resin (SEM) using FEI Inspect F50 high-resolution SEM with field
(1 and 2 wt%), the mixture was homogenized by mechanical emission gun and 1.2 nm resolution and energy dispersive
method for 3–5 min and by ultrasonication method (using an X-ray spectrometer (EDS). Tribological tests were performed
ultrasonic probe) for 15 min in steps of 5 min. Cork pow- on CETR UMT 3 (Universal Macro Materials Tester) block-
der was added to the obtained mixture at a weight ratio of on ring module, using 35 mm diameter steel role, under
1:5 (cork:resin), that was further mechanically homogenized. 10 N load, for 60 s at 1000 and 1500 rpm, testing three
The ternary mixtures were placed in an air oven at 65−70◦ C specimens for each sample. Thermal degradation behaviour
for 30 min to eliminate methanol solvent from the resin was followed by TG-DSC (Netzsch TG 449C STA Jupiter),
Bull. Mater. Sci. (2018) 41:28 Page 3 of 9 28

The graphic in figure 2 illustrates a linear increase of the

mixtures viscosity with nSiC weight content increase into the
PR. The standard deviation values for the viscosity average
values are situated between 0.3 and 1.4, suggesting that the
results are reproducible and also that the mixtures remained
homogenized during the experiment. This property is impor-
tant for the homogenization of cork powder into the nanofilled
resin mixtures to obtain the ablative type composites.
nSiC presence does not generate excessive viscosity inc-
Figure 2. Viscosity increase as a function of nSiC content into the rease and the values remain in the medium range. Too high
liquid PR. viscosity of the mixtures would hinder the uniform homog-
enization of the cork powder into the nanofilled polymeric
matrix that would lead to non-uniformity areas in the final
composites, while too low viscosity would lead to resin mate-
heating with 10 K min−1 from 25 to 900◦ C in 50 ml min−1 rial loss during curing–pressing stage that would generate low
Ar flow and from 900 to 1000◦ C in 50 ml min−1 dry air flow. matrix contents and air gasps into the composite and poor
Thermal shock tests were performed in air in a Nabertherm adhesion between the phases.
carbonization oven introducing the sample from room temper-
ature directly at 1100◦ C and maintaining it for three different
time lapses (30, 60 and 120 s), weight loss was measured as 3.2 Mechanical testing
a function of time.
Mechanical testing consisted of 3-point bending (flexural)
and compression tests performed both on control samples and
nSiC-filled samples. In the case of flexural testing, the load
3. Results and discussion was applied until reaching conventional deflection (deflection
equal to 1.5 × specimen thickness) according to the standard
3.1 Nanofilled resin viscosity measurements recommendations, but all tested specimens fractured before
this value was reached, suggesting the brittle nature of the
Viscosity measurements were performed at 25◦ C (using the materials, as the standard indicates.
thermostat bath that the viscometer is equipped with) on the Figures 3 and 4 present the stress–strain curves obtained
liquid PR with and without nSiC filler, after ultrasonication during the 3-point bending and compressive testing.
of the mixtures. Using the Ubbelohde viscometer, suitable for The curves allure and strain values lower than 5% also
polymeric solutions [26], minimum three measurements were suggest the brittle nature of the materials.
performed for each sample. The kinematic viscosity was cal- Table 1 presents the average values of the flexural and com-
culated as a ratio between the capillary constant K (expressed pressive properties obtained after testing, the results illustrate
in mm2 s−1 ) and the mean flow time (expressed in seconds) that these properties are influenced by nSiC nanofiller pres-
[27]. ence and content in the PR/cork composites.

Figure 3. Stress–strain curves during 3-point bending test.

28 Page 4 of 9 Bull. Mater. Sci. (2018) 41:28

Figure 4. Stress–strain curves during compression test.

Table 1. Mechanical properties of bending and compression of PR/nSiC/cork composites.

Flexural strength Flexural modulus Strain Compressive Compressive

Sample (MPa) (MPa) (%) strength (MPa) modulus (MPa)

PR/cork 10.1 ± 0.24 918 ± 15.3 1.12 19.68 ± 0.69 342.5 ± 20.9
PR+1% nSiC/cork 12.93 ± 0.15 1145 ± 18.8 1.03 24.65 ± 0.69 553 ± 29.3
PR+2% nSiC/cork 10.63 ± 0.49 1106 ± 18.9 0.91 21.06 ± 0.62 505.8 ± 15.5

nSiC addition generates strength and modulus increase with the addition of 1% by weight nanoparticles into the
compared with control sample (PR/cork) both under flex- phenolic matrix, the additional content up to 2% by weight not
ural loading as well as under compressive loading. It can being able to further interact with the resin. This issue along
be observed that 1% nSiC content generates more signifi- with the higher viscosity of the 2%-based samples contributes
cant properties, including increase than higher content of 2%. in hindering the uniform dispersion and homogeneity of the
Compared with the control sample, PR + 1% nSiC/cork shows materials, therefore, leading to less homogeneous structures.
28% higher flexural strength and 25% higher flexural modu- The structure of the PR/nSiC/cork composites was anal-
lus, while PR+2% nSiC/cork shows only 5% higher flexural ysed by SEM, further presented.
strength and 20% higher flexural modulus. The same trend is
observed in the case of compressive testing, 1% nSiC gen- 3.3 SEM analysis
erates 25% higher strength and 61% higher modulus, while
2% generates 7 and 48%, respectively, higher strength and SEM analyses were performed in the fracture cross-section
modulus. of the mechanically tested materials to visualize the interface
The possible cause for the lower increments of 2% nSiC- between the cork phase and the PR matrix, as well as the dis-
based samples, compared to the ones generated by lower persion of the nSiC nanoparticles into the phenolic matrix.
content could be that this higher content generates more The SEM images of the three samples registered at different
agglomeration areas that act as stress concentration sites that magnification levels are shown in figure 5. PR/cork sample
influence mechanical behaviour and properties. The positive is illustrated in figure 5a–c, PR+1% nSiC/cork in figure 5d–f
effect of 1% nSiC could be associated with good embedment and PR+2% nSiC/cork in figure 5g–i. At lower magnifica-
of the nanoparticles into the resin, generating a homoge- tion levels (×1000), in all samples (figure 5a, d, g), it can
nous structure of the nanofilled matrix and therefore, of the be observed that the simple or nanofilled resin is distributed
final composite. This phenomenon was observed also in the on the analysed area, covering at a high extent the cellular
case of nanocomposites based on PR and nSiC nanofiller structure of the cork. Medium magnification levels of ×5000
studied in the previous work [23]. According to the results illustrate clearly the cells that compose the structure of the
presented in the mentioned study, FTIR analysis suggests that cork, and it can be observed that the resin infiltrated into the
the maximum interaction between the resin and nSiC occurs inner structure of the cork cells. In figure 5e, it can be observed
Bull. Mater. Sci. (2018) 41:28 Page 5 of 9 28

Figure 5. (a) PR/cork at ×1000, (b) PR/cork at ×5000, (c) PR/cork at ×20000, (d) PR+1% nSiC/cork at ×1000, (e)
PR+1% nSiC/cork at ×5000, (f) PR+1% nSiC/cork at ×20000, (g) PR+2% nSiC/cork at ×1000, (h) PR+2% nSiC/cork
at ×5000, (i) PR+2% nSiC/cork at ×20000.

that the nSiC nanoparticles embedded into the resin layer are the uniform dispersion of nSiC nanoparticles in the phenolic
present inside the cellular structure, while figure 5f shows matrix of the sample, while in the case of the sample with
that the nSiC nanoparticles are also uniformly dispersed in higher nSiC content (PR+2% nSiC/cork) that exhibited a
the matrix on the entire visualized area. It can be noticed decrease in mechanical performance (compared with PR+1%
that while PR+1% nSiC/cork sample illustrates visible dif- nSiC/cork) SEM images showed clear nanoparticles agglom-
ferences in terms of morphology compared with the unfilled eration areas.
sample, PR+2% nSiC/cork has a mixed nature morphology. Uniformly dispersed nanoparticles into the matrix of the
This aspect is highlighted by figure 5i that shows both areas PR+1% nSiC/cork composite are able to strength the matrix,
with high nanoparticles content as well as areas that present allowing better load transfer within the composite system and
the morphology of a simple polymer layer, similar to the one leading to higher mechanical performance.
visualized in the control sample in figure 5c.
In the case of 1% nanofiller sample, the uniform dispersion
of nSiC into the PR is confirmed by EDS analysis (figure 6) 3.4 Tribological testing
that illustrates a perfect distribution of Si and C elements on
the area, results prove that Si is present in 41%, while C in As expected, the addition of abrasive nSiC nanofiller gen-
23%. erates significant increase of friction coefficient, using both
Correlating SEM analyses of the fracture cross-section speed rate values. Considering the nSiC mentioned tribolog-
with the mechanical performance of the composites, it can ical nature, friction coefficient increases with nSiC content
be noticed that in the sample with the highest mechanical in the composite. At 1000 rpm, compared with the PR/cork
performance (PR+1% nSiC/cork) SEM analysis confirmed sample with no nanometric agent, friction coefficient of the
28 Page 6 of 9 Bull. Mater. Sci. (2018) 41:28

Figure 6. (a) EDS analysis of PR+1% nSiC/cork cross-section and elemental distribution map of C and Si; and
(b) EDS spectra of the analysed area.

of the PR/nSiC/cork materials, it is worth mentioning that

besides the friction coefficient increase generated by the nSiC
nanoparticles, cork agent imprints even higher friction coef-
ficient increments, due to its well-known tribological nature.
The obtained results show that the materials could be used
as high friction materials in abrasive applications, due to the
improved tribological properties.

3.5 TG-DSC analysis

Thermogravimetry-differential scanning calorimetry (TG-

DSC) analysis was performed to evaluate the thermal behavi-
Figure 7. Friction coefficient average values of PR/nSiC/cork our of the obtained materials during controlled, linear
tested at 1000 and 1500 rpm. temperature increase. TG analysis was performed in inert
atmosphere (Ar) from room temperature to 900◦ C and in air
from 900 to 1000◦ C, to perform the combustion of the car-
nanofilled materials increased by 25 and 39%, respectively, bonaceous mass resulted in the previous stage.
for 1- and 2%-based samples. At 1500 rpm, the increments Figure 8a illustrating 25−900◦ C range shows that the
were by 28 and 33% for 1% and 2% nSiC contents into the mass loss occurs smoothly between 100 and 300◦ C, proba-
matrix compared to the control sample (figure 7). bly corresponding to organic compounds decomposition and
The results presented in the previous work of the authors the highest mass loss percentage occurs between 320 and
[23] that studied PR/nSiC matrix as self-standing materials 700◦ C. TG curves between 25 and 900◦ C illustrate the fact
showed the same overall trend in friction coefficient vari- that nSiC addition leads to an increase in the initial tempera-
ation when adding nSiC nanoparticles, the abrasive nature ture of the degradation process, and also, the control sample
of this nanofiller generating higher values of the friction shows a higher mass loss corresponding to the same tem-
coefficient compared to the unfilled resin. Comparing the tri- perature. TG curves in the 900−1000◦ C range (figure 8b)
bological properties of the PR/nSiC matrix with the properties illustrate that the sample with no nanofiller suffers a sharper
Bull. Mater. Sci. (2018) 41:28 Page 7 of 9 28

Figure 8. TG curves registered in (a) Ar flow between 25 and 900◦ C; and (b) air flow between 900 and 1000◦ C.

Figure 9. DSC graphs of the cork-based samples tested in inert

atmosphere between 25 and 900◦ C. Figure 10. Mass loss percentage of the thermal shock tested sam-
ples compared to the virgin samples, after different dwell periods at
1100◦ C.

weight loss, 3.24% residual mass is obtained starting from

940◦ C, while nanofilled samples’ corresponding curves have protection agent. In the high temperature region from 600 to
a smooth evolution up to 999.4◦ C. The residual mass of the 900◦ C, one can observe that the 2% content of nSiC nanopar-
PR+2% nSiC/cork is much higher than that of the control sam- ticles is able to diminish the effect of thermal degradation.
ple and 1% nSiC-based sample, which was expected as nSiC
compound with much higher thermal resistance compared to 3.6 Thermal shock test
the other phases, is present in higher content. Although the
residual mass increases with nSiC content as expected, but the Thermal shock test was performed to evaluate the mass loss
increase is not proportional. This suggests that the residual function of treatment period at 1100◦ C and test the abla-
mass does not correspond totally to the larger nSiC quantity, tive capacity of the obtained materials. Figure 10 illustrates
but it contains composite mass, indicating that the thermal the mass loss percentage of all the 3 samples (PR/cork,
stability of the composite is improved. PR+1% nSiC/cork and PR+2% nSiC/cork) after the three
DSC curves (figure 9) illustrate that thermal degradation dwell periods (30, 60 and 120 s) at 1100◦ C, compared with
of the nanofilled samples starts later than the control sample. the virgin samples. Two important trends are observed. As
Also, the control sample curve slope is higher, suggesting that expected, by increasing the thermal treatment time, the sam-
the exothermic effect is stronger. In the case of the nanofilled ples mass decreases, due to the decomposition of the organic
samples, the degradation process is delayed and the curves are compounds (shown by DSC) from the composite chemical
smoother, due to the nSiC presence, which acts as a thermal structure. Analysing nSiC-based samples, it can be observed
28 Page 8 of 9 Bull. Mater. Sci. (2018) 41:28

Figure 11. Samples before thermal shock and after 30 s at 1100◦ C, after 60 s at 1100◦ C, after 120 s at 1100◦ C.

that mass loss decreases as nanofiller content increases, due as a protection agent for the PR/cork composites, resulting
to the excellent thermal resistance [28] of this compound. into less damaged samples after thermal shock, aiding the
The nSiC nanoparticles act as thermal protection agent for material to maintain its integrity and suffer lower mass loss.
the cork-based composite, enhancing its ablative properties. TG-DSC results are in accordance with thermal shock test, as
These results are in accordance with TG analysis results con- the 2% nSiC-based samples present a non-linear increase of
cerning residual mass corresponding for each sample. the residual mass (function of nSiC content), suggesting that it
Figure 11 illustrates the material consumption when ther- corresponds to a composite residue. This indicates that nSiC is
mal treatment time increases. After 120 s at 1100◦ C, the able to act as a thermal barrier agent, preventing the combus-
unfilled PR/cork samples suffer rather high extent structure tion propagation in the composite. The results obtained in this
degradation, fracturing into two parts. By analysing the 1 and study sustain this type of nanocomposite material as potential
2% nSiC-filled samples appearance, none of them fractured candidate for thermal protection (i.e., ablative) application in
completely, and the sample with higher nanoparticles content aeronautic and aerospace industry.
shows fewer cracks than the lower content sample. Overall,
it can be observed that the nanofilled samples do not suf-
fer extended degradation of the structure, and the materials Acknowledgement
maintain their integrity, which recommends them as potential
candidates for thermal protection (ablative) applications. This work has been funded by the Sectorial Operational Pro-
gramme Human Resources Development 2007–2013 of the
Ministry of European Funds through the Financial Agreement
4. Conclusions POSDRU/159/1.5/S/134398.

The study presents the obtaining and characterization of cork-

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